5. Concentric Nebulizers
Sample solution introduction at rate of
between 0.01 and 3 mL/min
Microconcentric nebulizer (0.01â0.1
mL/min)
Cannot handle high total dissolved salts
(TDS 0.25% m/v solids)
5
7. High Solid Nebulizers
âą Very resistant to salting out
âą Suspended particles are presentV groove
âą Relatively high
Gas Pressure
âą Materials of construction that
resist hydrofluoric acid and
caustic attack.
Construction
7
8. Ultrasonic Nebulizers
These nebulizers use an ultrasonic generator at a frequency of between 200 kHz and 10 MHz to
drive a piezoelectric crystal.
Generation of Pressure
Desolvation
Condensation of particle
8
9. Spray Chambers
The purpose of the spray chamber is to remove droplets produced by the nebulizer that are >8ÎŒm
in diameter
Faster wash out time depends on wettability of glass
Water-cooled spray chambers may be used for volatile organic solvents
They are externally cooled for thermal stability of the molecule
Important advantage: to reduce oxide species, reduce solvent loading
9
10. Double pass Spray Chambers
Larger droplets emerge from the tube and exits
via drain tube
Liquid in the drain tube is kept at positive
pressure
Small droplets backs between outer wall and
central tube and emerges from spray chamber
10
11. Cyclonic spray chambers
Operates by centrifugal force
Vortex produced by tangential flow of sample and argon
gas inside the chamber
Larger droplets impinge on the wall and fall out through
drain
Chilled spray chambers
11
12. Laser ablation ICP-MS
Nd:YAG (neodymium doped yttrium
aluminum garnet crystal) laser.
Ablation chamber or cell, which is purged
with argon
UV beam diameter adjusted so that
âspotâ sizes from <5ÎŒm to 300ÎŒm
12
18. The Lens System - Focusing
Ions
Ion lens is positioned immediately behind the interface
Ions are passed through a positively charged metallic cylinder that
acts as a focusing lens
Ions get repelled due to similar charge
18
19. Collision cell and Reaction Cell
Used to remove polyatomic
interferences
Interferent ion will collide more
frequently with the inert gas (helium)
atoms than will the analyte ion, due to
its larger size
Each of these collisions removes a
certain amount of the kinetic energy
possessed by the ion
Collision
cell
Advantage of exothermic (fast) and
endothermic (slow) reactions.
An active gas, (like ammonia),
Reaction
cell
19
20. Ion deflector devices- Quadrupole Mass
Analyser
10 cm to 20 cm long
Mass analyser separates ions based
on the stability of their flight
trajectories through an oscillating
electric field in the quadrupole.
Triple Quadrupole System
20
22. Application
ï±Simple metal analysis during metal based drug development
ï±Impurity limit tests
ï±Metals present in Active Pharmaceutical Ingredients
ï±Quality Control Tests of natural products for toxic impurities testing
ï±Monitoring metabolites of an administered drug
ï±Detection of metal impurities from leachable packaging material
ï±For elemental speciation
ï±Pharmaceutical Waste Water monitoring
22
25. Sample introduction system other than ICP-MS
Hildebrand grid nebulizer (HGN)
High-speed argon gas emanating from the hole
shears the sheet of liquid into small droplets.
High velocity argon forces the liquid through
the tiny openings
V-groove allows the liquid to contact the
entire perimeter of the inner platinum grid.
High tolerance to dissolved solids
25
26. Hydride generator
Chemical reaction in generation of Hydride
NaBH4 + 3H2O + HCl H3BO4 + NaCl + 8H
8H + Em+ EHn + H2 (excess)
HG is a very effective sample introduction technique for
elements like arsenic, bismuth, germanium, lead,
antimony, selenium, tin, and tellurium.
26
27. Electrothermal vaporisation
High melting
point material
âą Graphite furnaces or other electrothermal devices,
such as carbon rods, carbon cups, graphite tubes,
tungsten wire
Current
programming
âą Low current is applied to evaporate sample solvent
and small portion of sample is vaporized by high
current
Introduction
into ICP
âą Dense cloud of the analyte vapor swept into the
centre of the plasma by a flow of argon gas.
27
28. Detection of emission
Concave grating placed on a Rowland circle
If the source of light and the grating are placed on the
circumference of a circle, and the circle has a diameter
equal to the radius of curvature of the grating, then the
spectrum will always be brought to a focus on the circle.
One entrance slit: for introduction of the source
radiation, multiple exit slits : around the circle at the
analytical wavelengths of interest.
No any collimating or focusing lenses or mirrors
28
29. Echelle grating coupled with a prism
order-sorting device
Echelle Polychromator
The echelle grating
is a coarsely ruled
grating, typically
having a groove
density of 70
grooves per mm, so
d(grooveâs spacing)
0.014 mm.
The efficiency of
the grating for a
given wavelength
at its optimum
order can be as
high as 65% at free
spectral range of
given order
Free spectral range
is smaller for
higher orders
hence spectral
overlaps occurs.
Overlap is sorted
by Order- Sorting
Prism.
29
30. Photomultiplier Tube
Cathode
âą Cathode: large surface area, vertical, hollow ââhalf cylinderââ
made up of alkali metal oxide
âą Photoemissive material at 1000 V
Anode
âą Anode: Collection grid
âą Fixed to ground potential
Dynodes
âą Up to 14 secondary emission dynodes placed between the
cathode and the anode potentials
âą that are successively more negative, by about 100V per dynode
30
31. Array detectors
Circular Optical System
âą Based upon a Rowland circle design
âą Provides total wavelength coverage from 120 to 800 nm, with
resolution on the order of 0.009 nm
Segmented array charge-coupled device detector
âą Over 200 small subarrays of 20â80 pixels each are used
âą Positioned along the two-dimensional focal plane of an echelle
polychromator
31
33. Applications
ï±Determination of metals in biological fluids (blood. urine)
ï±Environmental Analysis: Trace metals and other elements in water, soil and plants
ï±Pharmaceuticals: Traces of catalyst used
ï±Industry: Trace metal analysis in raw material
ï±Forensic science: Toxicological determination
33
34. Comparison between ICP-OES and ICP-
MS
ICP-OES ICP-MS
Sample introduction for solution of inorganic salt is
rapid and convenient
Sample introduction of inorganic salt can be difficult
(generally not volatile)
Sample introduction is at atmospheric pressure Requires reduced pressure sample introduction
Relatively large amount of dissolved solids can be
tolerated
Limited to less amount of dissolved solids by
conventional method (<1%)
Complicated spectra with frequent spectral overlap Relatively simple spectra
Moderate sensitivity (ppm to ppb range) Excellent sensitivity (ppb to ppt range)
Isotope ratio cannot be determined Isotope ratio determination possible
34
37. 20 tablets coming from one batch (containing MDMA) and 20 other tablets coming from another
batch (containing MDEA) were used
The variation depends on the element analysed. The mean variation was found to be 20% for
ICP/AES and 25% for ICP/MS. Therefore, these relative standard deviations represents the
variation within batch including the instrument and quantification errors.
RELATIVE STANDARD DEVIATIONS FOR ICP/MS AND ICP/AES
37
Editor's Notes
https://www.slideshare.net/AakratiGupta1/icpms
First, stabilizing the spray chamber at any temperature reduces temperature
related signal drift. Secondly, many analysts have found that spray chamber
temperature along with other parameters, particularly nebulizer gas flow, can
be optimized to minimize oxide formation in the plasma.
Though the fundamental dimensions are all essentially the same (sample
cone with shallow angle, skimmer cone with acute angle), each manufacturer
has designed the coneâs critical dimensions to their own unique specifications
(orifice diameter, hole depth, material composition, etc.).
Radial view
Plasma is operated in a vertical orientation, and the analytical zone is observed from the side of the plasma
Axial View
Plasma is rotated to a horizontal position and the ICP is observed from the end of the plasma.
Better sensitivity than radial view
Dual view
To optimize the appropriate configuration for the type of sample without the expense of two separate
Isotope fingerprinting: Isotope ratio mass spectrometry (IRMS) is used in product authentication to establish the origin of food and beverages. On the basis of stable isotope fingerprints from samples or in specific compounds, this approach may differentiate pharmaceutical products by manufacturer and production batch.
Multielement Analysis: